X射线荧光光谱法测定钒渣、钒渣熟料和提钒尾渣中主次组分

以四硼酸锂-碳酸锂为熔剂,碘化铵做脱模剂,熔融法制备样品,建立了X射线荧光光谱法(XRF)测定钒渣、钒渣熟料、提钒尾渣中二氧化硅、三氧化二铝、氧化钙、氧化镁、氧化锰、五氧化二钒、氧化铬、磷、二氧化钛和全铁的分析方法。试验表明,在试样量为0.25 g、稀释比(m_样品∶m_熔剂)为1∶20、脱模剂用量为20 mg时熔样效果最佳。采用经验系数法对基体效应进行校正及谱线重叠干扰校正,测定钒渣样品各组分的相对标准偏差(RSD,n=10)在0.10%~1.9%之间,检出限在35~460 μg/g之间。用标准物质和实际样品验证,测定结果与标准物质认定值和实际样品湿法测定值相符,能够满足日常分析的要求。

Determination of major and minor components in vanadium slag,vanadium slag clinker and vanadium tailings by X-ray fluorescence spectrometry

The sample was prepared by fusion method using lithium tetraborate-lithium carbonate as flux and ammonium iodide as releasing agent. The analysis method of silicon dioxide, aluminum oxide, calcium oxide, magnesium oxide, manganese oxide, vanadium pentoxide, chromium oxide, phosphorus, titanium dioxide and total iron in vanadium slag, vanadium slag clinker and vanadium tailings by X-ray fluorescence spectrometry(XRF) was established. The results showed that the sample fusion results were best under the following conditions: the sample mass was 0.25 g; the dilution ratio (m_Sample∶m_Flux) was 1∶20; the dosage of release agent was 20 mg. The empirical coefficient method was used for the correction of matrix effect and the spectral overlapping interference. The relative standard deviation (RSD, n=10) of components in vanadium slag samples was between 0.10% and 1.9%. The detection limits were between 35 μg/g and 460 μg/g. The proposed method was verified using the certified reference materials and actual samples. The found results were consistent with the certified values and those of actual samples obtained by wet method. The proposed method could meet the requirements of routine analysis.